Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate)

X. Jiang, V.G.R. Lima, P.J. Schoenmakers

Research output: Contribution to journalArticleAcademicpeer-review

34 Citations (Scopus)

Abstract

The separation of telechelic poly(methyl methacrylate) (PMMA) prepolymers based on the number of end-groups under critical liquid chromatography (LC) conditions has been studied using a bare-silica column, which can interact with polar functional groups. The critical solvent compositions for non-functional, mono-functional and bi-functional PMMAs were determined in normal-phase LC using mixtures of acetonitrile and dichloromethane (DCM) of varying composition as the mobile phase. The telechelic prepolymers were successfully separated according to hydroxyl (OH) functionality (with zero, one, or two OH groups, respectively) under the critical conditions, in which fast (5 min), base-line separations were obtained independent of molecular weight. Changing the column temperature, flow rate, and mobile-phase composition within a certain range did not affect the functionality separation. Therefore this isocratic LC separation method is quite robust. Evaporative light-scattering detector (ELSD) calibration curves were used for the quantitative analysis of functional PMMA prepolymers.
Original languageEnglish
Pages (from-to)19-27
JournalJournal of Chromatography, A
Volume1018
Issue number1
DOIs
Publication statusPublished - 2003

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Polymethyl Methacrylate
Liquid Chromatography
Liquid chromatography
Liquids
Methylene Chloride
Chemical analysis
Silicon Dioxide
Hydroxyl Radical
Calibration
Molecular Weight
Phase composition
Light scattering
Functional groups
Light
Temperature
Molecular weight
Flow rate
Detectors

Cite this

Jiang, X. ; Lima, V.G.R. ; Schoenmakers, P.J. / Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate). In: Journal of Chromatography, A. 2003 ; Vol. 1018, No. 1. pp. 19-27.
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Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate). / Jiang, X.; Lima, V.G.R.; Schoenmakers, P.J.

In: Journal of Chromatography, A, Vol. 1018, No. 1, 2003, p. 19-27.

Research output: Contribution to journalArticleAcademicpeer-review

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AU - Lima, V.G.R.

AU - Schoenmakers, P.J.

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N2 - The separation of telechelic poly(methyl methacrylate) (PMMA) prepolymers based on the number of end-groups under critical liquid chromatography (LC) conditions has been studied using a bare-silica column, which can interact with polar functional groups. The critical solvent compositions for non-functional, mono-functional and bi-functional PMMAs were determined in normal-phase LC using mixtures of acetonitrile and dichloromethane (DCM) of varying composition as the mobile phase. The telechelic prepolymers were successfully separated according to hydroxyl (OH) functionality (with zero, one, or two OH groups, respectively) under the critical conditions, in which fast (5 min), base-line separations were obtained independent of molecular weight. Changing the column temperature, flow rate, and mobile-phase composition within a certain range did not affect the functionality separation. Therefore this isocratic LC separation method is quite robust. Evaporative light-scattering detector (ELSD) calibration curves were used for the quantitative analysis of functional PMMA prepolymers.

AB - The separation of telechelic poly(methyl methacrylate) (PMMA) prepolymers based on the number of end-groups under critical liquid chromatography (LC) conditions has been studied using a bare-silica column, which can interact with polar functional groups. The critical solvent compositions for non-functional, mono-functional and bi-functional PMMAs were determined in normal-phase LC using mixtures of acetonitrile and dichloromethane (DCM) of varying composition as the mobile phase. The telechelic prepolymers were successfully separated according to hydroxyl (OH) functionality (with zero, one, or two OH groups, respectively) under the critical conditions, in which fast (5 min), base-line separations were obtained independent of molecular weight. Changing the column temperature, flow rate, and mobile-phase composition within a certain range did not affect the functionality separation. Therefore this isocratic LC separation method is quite robust. Evaporative light-scattering detector (ELSD) calibration curves were used for the quantitative analysis of functional PMMA prepolymers.

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